反应详情

Dissolve 3,5-dichloroaniline (10 g, 61.5 mmol) in 1:1 acetic acid/methylene chloride (200 mL). Add N-iodosuccinimide (16.9 g, 61.5 mmol) as a solid and stir at room temperature in the absence of light for 8 hours. Pour the solution into saturated sodium hydrogen carbonate (200 mL) and extract into methylene chloride (100 mL). Wash with saturated sodium hydrogen carbonate (200 mL), dry (MgSO4) and evaporate the solvent in vacuo. Purify by silica gel chromatography to give the title compound (8.1 g, 45%); mp 61°-63° C.

1. extractionextract into methylene chloride (100 mL)
2. washWash with saturated sodium hydrogen carbonate (200 mL)
3. dry with materialdry (MgSO4)
4. customevaporate the solvent in vacuo
5. customPurify by silica gel chromatography